WO2018221929A1 - 이차 전지용 전극의 기공 분포 측정 방법 - Google Patents
이차 전지용 전극의 기공 분포 측정 방법 Download PDFInfo
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- WO2018221929A1 WO2018221929A1 PCT/KR2018/006076 KR2018006076W WO2018221929A1 WO 2018221929 A1 WO2018221929 A1 WO 2018221929A1 KR 2018006076 W KR2018006076 W KR 2018006076W WO 2018221929 A1 WO2018221929 A1 WO 2018221929A1
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- Prior art keywords
- electrode
- secondary battery
- pores
- binder
- negative electrode
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- 239000011148 porous material Substances 0.000 title claims abstract description 143
- 238000009826 distribution Methods 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000011230 binding agent Substances 0.000 claims description 59
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 51
- 229910052710 silicon Inorganic materials 0.000 claims description 51
- 239000010703 silicon Substances 0.000 claims description 51
- 229920000642 polymer Polymers 0.000 claims description 37
- 239000000463 material Substances 0.000 claims description 36
- 230000003595 spectral effect Effects 0.000 claims description 28
- 238000010884 ion-beam technique Methods 0.000 claims description 18
- 238000004043 dyeing Methods 0.000 claims description 17
- 238000000992 sputter etching Methods 0.000 claims description 16
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 13
- 239000007772 electrode material Substances 0.000 claims description 13
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 239000004020 conductor Substances 0.000 claims description 8
- -1 polydimethylsiloxane Polymers 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 230000001678 irradiating effect Effects 0.000 claims description 6
- 150000002908 osmium compounds Chemical class 0.000 claims description 4
- 150000003304 ruthenium compounds Chemical class 0.000 claims description 3
- 229920000548 poly(silane) polymer Polymers 0.000 claims description 2
- 229920001709 polysilazane Polymers 0.000 claims description 2
- 229920001296 polysiloxane Polymers 0.000 claims description 2
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 34
- 238000013507 mapping Methods 0.000 description 26
- 239000000470 constituent Substances 0.000 description 21
- 238000004626 scanning electron microscopy Methods 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 13
- 229910052762 osmium Inorganic materials 0.000 description 8
- SYQBFIAQOQZEGI-UHFFFAOYSA-N osmium atom Chemical compound [Os] SYQBFIAQOQZEGI-UHFFFAOYSA-N 0.000 description 8
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 6
- 239000011149 active material Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 5
- 239000007773 negative electrode material Substances 0.000 description 5
- 239000003086 colorant Substances 0.000 description 4
- 239000004593 Epoxy Substances 0.000 description 3
- FDLZQPXZHIFURF-UHFFFAOYSA-N [O-2].[Ti+4].[Li+] Chemical compound [O-2].[Ti+4].[Li+] FDLZQPXZHIFURF-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 239000006182 cathode active material Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 150000001993 dienes Chemical class 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000004445 quantitative analysis Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- 229920005822 acrylic binder Polymers 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 229910021383 artificial graphite Inorganic materials 0.000 description 1
- 239000003013 cathode binding agent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000011883 electrode binding agent Substances 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910021385 hard carbon Inorganic materials 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- 238000007557 optical granulometry Methods 0.000 description 1
- 229910000487 osmium oxide Inorganic materials 0.000 description 1
- JIWAALDUIFCBLV-UHFFFAOYSA-N oxoosmium Chemical compound [Os]=O JIWAALDUIFCBLV-UHFFFAOYSA-N 0.000 description 1
- 230000021715 photosynthesis, light harvesting Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229910001925 ruthenium oxide Inorganic materials 0.000 description 1
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 1
- 229920005573 silicon-containing polymer Polymers 0.000 description 1
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Definitions
- the present invention relates to a method for measuring the pore distribution of an electrode for secondary batteries that can easily measure the pore distribution inside the electrode for secondary batteries.
- the secondary battery is largely composed of an electrode, a separator and an electrolyte, and the electrode is classified into a cathode and an anode. Since constituent materials such as an active material, a conductive material, and a binder are three-dimensionally distributed in the electrode, many pores exist in these gaps. The pores present in the electrode are filled with the electrolyte in the secondary battery to become a passage of ions or the like. Therefore, it is important to accurately analyze the distribution of pores in the electrode because the size, number, and distribution of the pore affect the diffusivity of the ions and the secondary battery performance.
- Patent Document 1 Republic of Korea Patent Publication No. 2014-0132956
- the present invention relates to a method for measuring the pore distribution of an electrode for a secondary battery that can easily analyze the distribution of pores in the electrode by clearly distinguishing the electrode internal constituent material and the pores.
- One embodiment of the present invention comprises the steps of preparing an electrode for a secondary battery comprising an electrode active material, a binder and a conductive material; Impregnating a polymer including silicon into the secondary battery electrode to fill the polymer including the silicon in internal pores of the secondary battery electrode; Preparing an electrode cross-section sample by irradiating an ion beam of an ion milling device on the secondary battery electrode; Detecting silicon present in the sample of electrode cross-section using an energy dispersive spectral element analyzer; And determining a distribution of pores by analyzing an image to which points of silicon detected by the energy dispersive spectral element analyzer are mapped.
- the pore distribution in the electrode may be confirmed by clearly distinguishing the constituent material and the pores of the electrode, and thereby accurately predicting the performance of the electrode for the secondary battery.
- the pores in the electrode can be more clearly distinguished by dyeing the binder.
- FIG. 1 is a view showing the ion milling apparatus used in the step of preparing an electrode cross-section sample according to an embodiment of the present invention.
- FIG. 2A is a cross-sectional view of two secondary battery negative electrodes
- FIG. 2B is a graph illustrating charging characteristics of the two secondary battery negative electrodes.
- Figure 3a is a view showing the EDS mapping image of the pores of the negative electrode cross-section sample obtained using energy-dispersive X-ray spectroscopy (EDS) according to an embodiment of the present invention
- Figure 3b is a pore of the negative electrode cross-section sample A diagram showing an image extracted by applying the EDS mapping image to image processing.
- EDS energy-dispersive X-ray spectroscopy
- FIG. 4A illustrates an EDS mapping image of a binder of a negative electrode cross-sectional sample obtained using an EDS according to an exemplary embodiment of the present invention
- FIG. 4B illustrates an EDS mapping image of a binder of a negative electrode cross-section sample applied to image processing. The extracted image is shown.
- FIG. 5A is a scanning electron microscope (SEM) photograph of the negative electrode cross-section sample prepared in Example 1
- FIG. 5B is a SEM photograph of the negative electrode cross-section sample prepared in Example 2
- FIG. 5C is a negative electrode cross-section prepared in Comparative Example 1
- a SEM photograph of the sample
- FIG. 5D is an SEM photograph of the negative electrode cross section sample prepared in Comparative Example 2
- FIG. 5E is an SEM photograph of the negative electrode cross section sample prepared in Comparative Example 3.
- Figure 6a is a view showing the EDS mapping image of the negative electrode cross-sectional sample according to Example 1 and Example 2 of the present invention obtained using the EDS
- Figure 6b is a negative electrode cross-sectional sample according to Example 1 and Example 2
- the EDS mapping image is applied to image processing to show the extracted image.
- One embodiment of the present invention comprises the steps of preparing an electrode for a secondary battery comprising an electrode active material, a binder and a conductive material; Impregnating a polymer including silicon into the secondary battery electrode to fill the polymer including the silicon in internal pores of the secondary battery electrode; Preparing an electrode cross-section sample by irradiating an ion beam of an ion milling device on the secondary battery electrode; Detecting silicon present in the sample of electrode cross-section using an energy dispersive spectral element analyzer; And determining a distribution of pores by analyzing an image to which points of silicon detected by the energy dispersive spectral element analyzer are mapped.
- the pore distribution in the electrode may be confirmed by clearly distinguishing the constituent material and the pores of the electrode, and thereby accurately predicting the performance of the electrode for the secondary battery.
- the secondary battery electrode includes an electrode active material, a binder, and a conductive material.
- the secondary battery electrode may further include various additives capable of improving its performance.
- the electrode active material, the binder, and the conductive material are three-dimensionally distributed in the electrode for the rechargeable battery, and a plurality of pores may exist in the gap. That is, an electrode constituent material such as an electrode active material, a binder, a conductive material, and a plurality of pores may constitute the secondary battery electrode.
- the electrode active material, the binder, and the conductive material included in the secondary battery electrode a material commonly used in the art may be used without particular limitation.
- a diene binder such as carboxymethyl cellulose (CMC), butadiene, acrylic binder, or the like may be used as the binder.
- CMC carboxymethyl cellulose
- acrylic binder acrylic binder
- various types of carbon-based materials including artificial graphite, natural graphite, or hard carbon, non-carbon-based materials including silicon (Si) and lithium titanium oxide (Lithium Titanium Oxide: LTO) and the like can be used.
- Si silicon
- Lithium Titanium Oxide: LTO lithium titanium oxide
- the filling of the polymer including the silicon in the internal pores of the secondary battery electrode includes impregnating the polymer including silicon into the electrode for the secondary battery, and the polymer including silicon to the secondary. It may be to penetrate the pores of the battery electrode.
- Liquid polymers may be used as the polymer containing silicon. Using a liquid polymer containing silicon, it is possible to more effectively fill the polymer containing the silicon in the pores of the secondary battery electrode.
- the method of impregnating the polymer containing silicon in the pores of the secondary battery electrode may be carried out by a conventional method in the art.
- the polymer including silicon may be applied to the secondary battery electrode by applying the silicon-containing polymer onto the secondary battery electrode, or immersing the secondary battery electrode in the polymer solution containing silicon. Can be impregnated into the pores.
- FIG. 1 is a view showing the ion milling apparatus used in the step of preparing an electrode cross-section sample according to an embodiment of the present invention.
- a focused ion beam generated by an ion gun may be irradiated onto a surface of a sample through a mask.
- the electrode materials may be sputtered by irradiating an ion beam generated in an ion gun of an ion milling device on the secondary battery electrode.
- This can produce an electrode cross-section sample having a clean cross section without physical damage.
- the pores of the secondary battery electrode can be analyzed more precisely.
- the ion beam may be an argon ion beam.
- the said electrode cross-section sample can be manufactured more stably.
- the ion beam current of the ion milling device may be 100 ⁇ A or more and 250 ⁇ A or less. Specifically, the ion beam current of the ion milling device may be 110 ⁇ A or more and 150 ⁇ A or less, or 200 ⁇ A or more and 230 ⁇ A or less.
- the branch can manufacture an electrode cross-section sample. Through this, the analysis efficiency of the internal pores of the secondary battery electrode can be increased.
- the discharge current of the ion milling device may be 250 ⁇ A or more and 450 ⁇ A or less.
- the discharge current of the ion milling apparatus may be 370 ⁇ A or more and 450 ⁇ A or less, or 400 ⁇ A or more and 430 ⁇ A or less.
- the detecting of the silicon present in the electrode cross-section sample may determine a point where silicon exists in the electrode cross-section sample by using the energy dispersive spectral element analyzer.
- the polymer containing silicon is filled in the pores of the electrode for the secondary battery, it is possible to detect the silicon contained in the polymer filled in the pores by using the energy dispersive spectral element analyzer. Through this, it is possible to determine the location of the pores in the secondary battery electrode, the size, number, distribution, and the like of the pores.
- the pores formed in the gaps of the materials constituting the electrode may be a passage of ions, and the like, and the size, number, and distribution of pores present in the electrode may greatly affect the performance of the secondary battery.
- FIG. 2A is a cross-sectional view of two secondary battery negative electrodes
- FIG. 2B is a graph illustrating charging characteristics of the two secondary battery negative electrodes.
- FIG. 2A illustrates two secondary battery negative electrode cross-sections having the same total pore distribution but having different pore distributions on the upper and lower portions on the negative electrode cross-section of the secondary battery.
- the negative electrode 1 and the negative electrode 2 have the same distribution of 25% of the total pores on the same area.
- FIG. 2A in the case of the negative electrode 1, pores are similarly sized in the upper and lower portions on the negative electrode cross section, and are evenly distributed in the upper and lower portions.
- the pores present in the upper portion on the negative electrode cross section is larger than the pores present in the lower portion, there are more pores in the upper portion than the lower portion.
- FIG. 2B illustrates a state of charge (SOC) according to voltages applied to the negative electrodes 1 and 2. Referring to FIG.
- the negative electrode 2 having a larger pore size in the upper portion on the negative electrode cross section and more pores in the upper portion than the lower portion is compared to the negative electrode 1 in which pores of similar size are evenly distributed in the upper and lower portions on the negative electrode cross section. It turns out that the charging characteristic is excellent.
- the present invention by filling a polymer containing silicon in the pores of the secondary battery electrode, by detecting the silicon present in the electrode cross-sectional sample prepared from the secondary battery electrode, the material and the pores can be clearly distinguished, and the size, number, distribution, etc. of the pores can be easily confirmed.
- the material signal of the secondary battery electrode which may be generated by filling the polymer including the silicon in the pores of the electrode for the secondary battery, may be generated by the presence of the material of the secondary battery electrode on different focal planes at the bottom of the pore.
- the phenomenon which is detected can be prevented. Therefore, even when the electrode cross-section sample in which the polymer containing silicon is filled in the pores of the secondary battery electrode is observed with a scanning electron microscope, the constituent material of the pores and the secondary battery electrode can be distinguished.
- the constituent material and the pores of the secondary battery electrode is clearly distinguished, and the size, number, distribution, etc. of the pores are determined. It can be easily analyzed.
- the pores can be accurately analyzed and the distribution of the pores can be confirmed, and thus the secondary battery electrode and the secondary battery including the same The performance of can be predicted more effectively.
- the polymer containing silicon is polydimethylsiloxane (polydimethylsiloxane). It may include one or more selected from the group consisting of polysiloxane, polysilane, and polysilazane. Silicon may be included in a repeat unit of the polymer including silicon. The silicon component included in the polymer may maximize the contrast effect due to the atomic number difference, thereby clearly distinguishing the pores and the constituent material of the electrode for secondary batteries.
- the distribution of pores present in the secondary battery electrode and the size, number, location, etc. of the pores can confirm.
- the energy-dispersive X-ray spectroscopy may be used to attach to a scanning electron microscope.
- the energy dispersive spectral element analyzer is an analytical device that detects X-rays generated when an electron beam is irradiated onto a sample surface and measures components of the sample. There is an advantage to this.
- an energy dissipation type spectral element analyzer having an energy resolution of 5.9 keV or more and 136 keV or less and having a minimum detection limit of 0.1 wt% may be used.
- the silicon of the polymer filled in the pores of the secondary battery electrode can be detected more accurately.
- the energy dispersive spectral element analyzer may detect silicon of the polymer filled in the pores of the secondary battery electrode, and extract the EDS mapping image displaying the detected silicon spot.
- the location of the pores of the electrode for secondary batteries, the shape, size, number, distribution, and the like of the pores of the secondary battery electrode may be confirmed through the mapped image of the silicon.
- the determining of the pore distribution may include quantitatively analyzing the pore distribution of the secondary battery electrode.
- the EDS mapping image extracted by the energy dispersive spectral element analyzer may be applied to image processing to quantitatively analyze the pore distribution of each part of the electrode for secondary batteries.
- an image processing operation converts the EDS mapping image to black and white, and uses the partial brightness difference in the EDS mapping image converted to black and white to effectively remove pores and electrode constituents in the cross section of the sample of the electrode cross section. Can be distinguished. By distinguishing the pores of the electrode cross-section sample and the electrode constituent material, it is possible to quantitatively analyze the pore distribution for each part of the secondary battery electrode.
- the cross-section of the sample of the electrode cross-section prepared from the electrode for secondary batteries can be classified into upper, middle and lower, and each of the upper, middle and lower portions can be classified into smaller unit areas to precisely quantitatively analyze the pore distribution. Can be.
- pore distribution of the electrode for secondary batteries may be quantitatively analyzed, thereby including the secondary battery electrode.
- the performance of the secondary battery can be calculated in advance.
- Figure 3a is a view showing the EDS mapping image of the pores of the negative electrode cross-section sample obtained using energy-dispersive X-ray spectroscopy (EDS) according to an embodiment of the present invention
- Figure 3b is a pore of the negative electrode cross-section sample A diagram showing an image extracted by applying the EDS mapping image to image processing.
- EDS energy-dispersive X-ray spectroscopy
- an image of the cathode cross-section sample cross-section extracted by image processing may be classified into upper, middle, and lower regions.
- each region classified into upper, middle, and lower portions may be equally divided into three units from the upper direction to the lower direction to be divided into nine unit regions, and the pores of the negative electrode for secondary batteries may be quantitatively analyzed using the same.
- the step of preparing the electrode cross-sectional sample may further comprise the step of dyeing the binder.
- the dyeing may be performed before the step of filling the polymer containing silicon in the pores of the secondary battery electrode, or may be performed after the step of filling the polymer. Even when the electrode cross section sample is observed with a scanning electron microscope by dyeing the binder, the binder, the electrode active material, the pores, and the like can be distinguished from each other.
- the binder included in the secondary battery electrode by dyeing the binder included in the secondary battery electrode, the binder and the electrode active material, pores, etc. can be clearly distinguished, and thus the pores of the secondary battery electrode can be analyzed more precisely. Can be.
- the step of dyeing the binder may be dyed the binder with a dyeing material containing at least one of an osmium compound and a ruthenium compound.
- a dyeing material containing at least one of an osmium compound and a ruthenium compound.
- osmium oxide such as OsO 4
- ruthenium oxide such as RuO 4
- OsO as shown below in Scheme 14 it may be coupled by reacting with the double bond of butadiene.
- the osmium component included in the osmium compound can maximize the contrast effect due to the atomic number difference, so that the binder and the pores of the secondary battery electrode, the electrode active material, and the like can be clearly distinguished.
- the energy dispersive spectral element analyzer using the energy dispersive spectral element analyzer, detecting the dyeing material in the binder; And calculating an area ratio of the binder by analyzing an image to which the points of the dyeing material detected by the energy dispersive spectral element analyzer are mapped.
- osmium dyed in the binder may be detected by using the energy dispersive spectral element analyzer, and the spot of the detected osmium is displayed. EDS mapping image can be extracted. The area, location, distribution, etc. of the binder included in the secondary battery electrode may be grasped through the image in which the points of the osmium are mapped. Through this, it is possible to more accurately check the distribution of the pores present in the secondary battery electrode and the size, number, location, and the like of the pores.
- the step of calculating the area ratio of the binder by analyzing the image to which the point of osmium is mapped may include processing the EDS mapping image extracted by the energy dispersive spectral element analyzer.
- the area of the binder for each part of the secondary battery electrode can be quantitatively analyzed.
- the cross-section of the sample of the electrode cross-section prepared from the electrode for secondary batteries can be classified into upper, middle and lower, and each of the upper, middle and lower portions are classified into smaller unit regions to precisely area ratio of the binder. Can be calculated
- FIG. 4A illustrates an EDS mapping image of a binder of a negative electrode cross-sectional sample obtained using an EDS according to an exemplary embodiment of the present invention
- FIG. 4B illustrates an EDS mapping image of a binder of a negative electrode cross-section sample applied to image processing. The extracted image is shown.
- the constituent material of the negative electrode for a secondary battery that appears in dark colors and the binder that appears in brighter colors are clearly distinguished. You can check it.
- an image of the cathode cross section sample cross section extracted by image processing may be classified into upper, middle, and lower regions. In addition, each region classified into upper, middle, and lower portions may be divided into three unit regions from the upper direction to the lower direction, and classified into nine unit areas in total. Using this, the area of the binder of the negative electrode for secondary batteries can be quantitatively analyzed.
- the binder area ratio of the electrode for secondary batteries may be quantitatively analyzed using the mapping image extracted by the energy dispersive spectral element analyzer. Through this, it is possible to more accurately grasp the distribution of pores of the secondary battery electrode, and to calculate the performance of the secondary battery electrode and the secondary battery including the same in advance.
- the method of measuring pore distribution of a secondary battery electrode according to an exemplary embodiment of the present invention may be applied to a positive electrode and a negative electrode for a secondary battery.
- a secondary battery negative electrode (LG CHEM Co., Ltd.) was prepared, and polydimethylsiloxane (PDMS) was prepared as a polymer containing OsO 4 and silicon as the dyeing material.
- the prepared OsO 4 was used to dye the binder of the negative electrode for the secondary battery, and the negative electrode for the secondary battery was impregnated into the prepared PDMS to fill the negative electrode pores for the secondary battery with PDMS.
- an ion milling apparatus IM 4000, Hitachi Co., Ltd.
- IM 4000 Hitachi Co., Ltd.
- a focused argon (Ar) ion beam was irradiated with a focused argon (Ar) ion beam to the anode for the secondary battery to cut a surface to prepare a negative electrode cross-section sample having a clean cross section.
- discharge current was performed at 400 ⁇ A and ion beam current at 130 ⁇ A, and the gas flow was 1 cm 3 / min and was performed for 3 hours.
- a negative electrode cross section was prepared in the same manner as in Example 1, and in the state in which the binder of the negative electrode for the secondary battery was not dyed, the cross section of the negative electrode was the same as in Example 1 except that the pores of the negative electrode for the secondary battery were filled with polydimethylsiloxane. Samples were prepared.
- a negative electrode for a secondary battery was prepared in the same manner as in Example 1, except that the binder of the negative electrode for the secondary battery was dyed with OsO 4 , and the pores of the negative electrode for the secondary battery were filled with a polymer containing epoxy, in the same manner as in Example 1.
- a negative electrode cross section sample was prepared.
- a negative electrode was prepared in the same manner as in Example 1, except that the binder of the negative electrode for the secondary battery was not dyed and the pores of the negative electrode for the secondary battery were not filled with a polymer containing silicon. Sectional samples were prepared.
- a negative electrode cross-section sample was prepared in the same manner as in Example 1, except that the same negative electrode for the secondary battery was prepared as in Example 1, and the pores of the negative electrode for the secondary battery were filled with a polymer containing epoxy without dyeing the binder of the negative electrode for the secondary battery. was prepared.
- the negative electrode cross-sectional samples prepared in Examples 1, 2 and Comparative Examples 1 to 3 of the present invention were observed with a scanning electron microscope (SU8020, HITACHI Co., Ltd.), and SEM pictures were taken.
- FIG. 5A is a scanning electron microscope (SEM) photograph of the negative electrode cross-section sample prepared in Example 1
- FIG. 5B is a SEM photograph of the negative electrode cross-section sample prepared in Example 2
- FIG. 5C is a negative electrode cross-section prepared in Comparative Example 1
- a SEM photograph of the sample
- FIG. 5D is an SEM photograph of the negative electrode cross section sample prepared in Comparative Example 2
- FIG. 5E is an SEM photograph of the negative electrode cross section sample prepared in Comparative Example 3.
- a polymer containing silicon may be filled in the pores of the secondary battery electrode to clearly distinguish the pores and the negative constituent material, and the binder may be clearly distinguished by dyeing the binder of the secondary battery electrode. As a result, pores of the secondary battery electrode can be confirmed more precisely.
- the energy dispersive spectral element analyzer attached to the scanning electron microscope (SU8020, HITACHI Co., Ltd.) of the negative electrode cross-section sample prepared in Example 1, the silicon component of PDMS filled in the negative electrode pores for secondary batteries was detected, OsO 4 Dyed on Cathode Binder The osmium component of the dye was detected. Thereafter, an EDS mapping image showing the detected points of silicon and osmium was extracted. Thereafter, the extracted EDS mapping image was applied to image processing to extract an image for quantitative analysis of pores. At this time, an energy dispersion type spectral element analyzer having an energy resolution of 5.9 keV or more and 136 keV or less and having a minimum detection limit of 0.1 wt% was used.
- the silicon component of PDMS filled in the anode pores for secondary batteries is detected, and the EDS mapping image showing the detected silicon spot is extracted. It was. Thereafter, the extracted EDS mapping image was applied to image processing to extract an image for quantitative analysis of pores.
- Figure 6a is a view showing the EDS mapping image of the negative electrode cross-sectional sample according to Example 1 and Example 2 of the present invention obtained using the EDS
- Figure 6b is a negative electrode cross-sectional sample according to Example 1 and Example 2
- the EDS mapping image is applied to image processing to show the extracted image.
- Example 1 the pores, the negative electrode active material, and the binder were clearly distinguished from each other on the negative electrode cross-section sample, and in Example 2, the binder was not dyed to distinguish only the pores and the negative electrode active material. Confirmed that it can.
- the image of the cathode cross section sample cross section extracted by image processing may be classified into upper, middle, and lower regions, and each region classified into upper, middle, and lower regions may be divided into three regions from the upper direction to the lower direction.
- the pores of the negative electrode for secondary batteries were quantitatively analyzed by dividing into nine unit areas.
- Table 1 below describes the porosity, the negative electrode active material region, and the ratio of the binder region indicating the distribution of pores in each of the nine unit regions of the secondary battery negative electrode manufactured in Example 1, and in Table 2 below.
- the porosity of the area of each of the nine unit regions of the negative electrode for secondary batteries prepared in Example 2 and the ratio of the binder region were described.
- Example 1 in which the pores were impregnated with PDMS and the binder was dyed with OsO 4 was compared with Example 2, which did not dye the binder.
- Example 2 in which the binder was dyed the pore and the negative electrode active material were distinguished from the binder, so that the porosity in the unit region was smaller than that in Example 2, and through this, the porosity of the negative electrode for the secondary battery was more accurately confirmed. It can be seen that.
- the present invention it is possible to quantitatively analyze the pores, the active material and the binder present in the secondary battery electrode, thereby predicting the performance of the secondary battery using the secondary battery electrode.
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Abstract
Description
영역 | 상 | 중 | 하 | 평균 | ||||||
단위 영역 | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | |
음극활물질(%) | 65.1 | 59.6 | 57.2 | 61.0 | 58.7 | 60.3 | 59.8 | 54.4 | 57.4 | 59.3 |
바인더(%) | 0.7 | 2.1 | 2.0 | 2.5 | 1.7 | 3.1 | 1.1 | 1.4 | 1.3 | 1.8 |
공극률(%) | 34.2 | 38.3 | 40.8 | 36.5 | 39.6 | 36.6 | 39.1 | 44.2 | 41.3 | 38.9 |
영역 | 상 | 중 | 하 | 평균 | ||||||
단위 영역 | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | |
음극활물질(%) | 65.7 | 58.8 | 56.4 | 61.3 | 57.3 | 60.7 | 60.8 | 54.6 | 57.2 | 59.2 |
공극률(%) | 34.3 | 41.2 | 43.6 | 38.7 | 42.7 | 39.3 | 39.2 | 45.4 | 42.8 | 40.8 |
Claims (8)
- 전극 활물질, 바인더 및 도전재를 포함하는 이차 전지용 전극을 준비하는 단계;규소를 포함하는 고분자를 상기 이차 전지용 전극에 함침하여, 상기 이차 전지용 전극의 내부 기공에 상기 규소를 포함하는 고분자를 채우는 단계;이온 밀링 장치의 이온 빔을 상기 이차 전지용 전극에 조사하여 전극 단면 시료를 제조하는 단계;에너지 분산형 스펙트럼 원소 분석기를 이용하여, 상기 전극 단면 시료에 존재하는 규소를 검출하는 단계; 및상기 에너지 분산형 스펙트럼 원소 분석기에 의해 검출된 규소의 지점이 맵핑된 이미지를 분석하여 기공의 분포를 확인하는 단계;를 포함하는 이차 전지용 전극의 기공 분포 측정 방법.
- 청구항 1에 있어서,상기 규소를 포함하는 고분자는 폴리디메틸실록세인. 폴리실록세인, 폴리실레인 및 폴리실라제인으로 이루어진 군으로부터 선택되는 1종 이상을 포함하는 것인 이차 전지용 전극의 기공 분포 측정 방법.
- 청구항 1에 있어서,상기 전극 단면 시료를 제조하는 단계 전에,상기 바인더를 염색하는 단계를 더 포함하는 것인 이차 전지용 전극의 기공 분포 측정 방법.
- 청구항 3에 있어서,상기 바인더를 염색하는 단계는 오스뮴 화합물 및 류테늄 화합물 중 적어도 하나를 포함하는 염색재로 상기 바인더를 염색하는 것인 이차 전지용 전극의 기공 분포 측정 방법.
- 청구항 4에 있어서,에너지 분산형 스펙트럼 원소 분석기를 이용하여, 상기 바인더 내의 염색재를 검출하는 단계; 및상기 에너지 분산형 스펙트럼 원소 분석기에 의해 검출된 염색재의 지점이 맵핑된 이미지를 분석하여 바인더의 면적 비율을 계산하는 단계;를 더 포함하는 것인 이차 전지용 전극의 기공 분포 측정 방법.
- 청구항 1에 있어서,상기 이온 빔은 아르곤 이온 빔인 것인 이차 전지용 전극의 기공 분포 측정 방법.
- 청구항 1에 있어서,상기 이온 밀링 장치의 이온 빔 전류는 100 μA 이상 250 μA 이하인 것인 이차 전지용 전극의 기공 분포 측정 방법.
- 청구항 1에 있어서,상기 이온 밀링 장치의 방전 전류는 250 μA 이상 450 μA 이하인 것인 이차 전지용 전극의 기공 분포 측정 방법.
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KR20210007165A (ko) * | 2019-07-10 | 2021-01-20 | 주식회사 엘지화학 | 리튬 이차전지용 전극의 전극 활물질 깨짐율 분석 방법 |
US11334984B2 (en) | 2019-07-10 | 2022-05-17 | Lg Energy Solution, Ltd. | Analysis method for crack rate of electrode active material of electrode for lithium secondary battery |
KR102420242B1 (ko) | 2019-07-10 | 2022-07-13 | 주식회사 엘지에너지솔루션 | 리튬 이차전지용 전극의 전극 활물질 깨짐율 분석 방법 |
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EP3633359A1 (en) | 2020-04-08 |
KR20180130462A (ko) | 2018-12-07 |
US20200141841A1 (en) | 2020-05-07 |
KR102097613B1 (ko) | 2020-04-06 |
CN110352347A (zh) | 2019-10-18 |
EP3633359A4 (en) | 2020-06-24 |
JP2020507889A (ja) | 2020-03-12 |
CN110352347B (zh) | 2022-04-15 |
JP6860129B2 (ja) | 2021-04-14 |
EP3633359B1 (en) | 2024-06-12 |
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